偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定石膏中多组分含量  

Determination of Multi-component Content in Gypsum by Inductively Coupled Plasma Atomic Emission spectrometry with Lithium Metaborate-Lithium Tetraborate Fusion

作　　者：张丽萍 孙启亮 姚明星[1,2,3] 张宏丽 肖芳[1,2,3] 倪文山 ZHANG Liping;SUN Qiliang;YAO Mingxing;ZHANG Hongli;XIAO Fang;NI Wenshan(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou,Henan 450006,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou,Henan 450006,China;Key Laboratory for Polymetallic Ore Evaluation and Utilization,MNR,Zhengzhou,Henan 450006,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,郑州450006 [3]自然资源部多金属矿综合利用评价重点实验室,郑州450006

出　　处：《中国无机分析化学》2023年第7期741-747,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学基金青年基金资助项目(21806149,22106148)。

摘　　要：石膏在我国储量丰富,应用广泛,快速准确分析其成分含量对石膏资源的综合利用具有重要意义。针对酸溶法无法测定SiO_(2),碱熔法无法测定K_(2)O、Na_(2)O的问题,通过优化熔剂用量、熔融温度,建立了偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱法同时测定石膏中CaO、SO_(3)、Al_(2)O_(3)、Fe_(2)O_(3)、MgO、TiO_(2)、K_(2)O、Na_(2)O、SiO_(2)含量的方法。结果表明采用试样与偏硼酸锂-四硼酸锂混合熔剂质量比例1∶5,在铂金坩埚中1000℃熔融10 min,在超声条件下,于50 mL盐酸(10%)中浸取熔融物,能够有效分解试样而浸取待测组分。向标准溶液系列中加入偏硼酸锂-四硼酸锂-盐酸基体溶液以消除基体对测试结果的影响。各待测组分的校准曲线的相关性系数均大于0.999,方法检出限在3~292μg/g;分别对国家一级标准物质GBW03109a、GBW03110和实际样品进行测定,5次平行测试标准物质的相对标准偏差(RSD)在0.14%~8.9%,测定结果的相对误差在0.030%~8.9%,测试结果与标准值无显著性差异;实际样品中各成分测定值的RSD(n=5)为0.24%~8.8%。方法操作简单、准确度高、精密度好、检出限低,可以同时测定石膏中的多组分含量,能够为石膏资源综合利用、调查评价提供一定的技术支撑。Gypsum is abundant and widely used in China.Rapid and accurate analysis of its composition is of great significance for comprehensive utilization o f gypsum resources.In order to solve the problem that the acid solution method can not determine the silicon dioxide,and the alkali fusion method can not determine the potassium and sodium,after optimization of the solvent dosage,fusion temperature,a method for simultaneous determination of CaO,SO_(3),Al_(2)O_(3),Fe_(2)O_(3),MgO,TiO_(2),K_(2)O,Na_(2)O and SiO_(2)in gypsum was established by inductively coupled plasma atomic emission spectrometer with the lithium metaborate-lithium tetraborate fusion.The results showed that the sample was fused with the mixed solvent of lithium metaborate and lithium tetraborate at a ratio of 1∶5 in a platinum crucible at 1000℃for 10 minutes.After that,50 mL 10%hydrochloric acid ultrasonic leaching method can effectively decompose the sample and soak the elements to be measured.The influence of matrix on test results was eliminated by adding matrix into standard solution series.The correlation coefficients of calibration curves and calibration equations of the elements to be tested were all greater than 0.999.The detection limits of the elements to be tested ranged from 3-292μg/g,The national first-class standard substances GBW03109a,GBW03110 and actual samples were determined by the experimental method.The relative standard deviations of the five parallel tests of the reference materials ranged from 0.14%—8.9%,the relative error of the measurement results is between 0.030%—8.9%.There is no significant difference between the test results and the standard values.The RSD(n=5)of each component in the actual samples was 0.24%—8.8%.This method has the advantages of simple operation,high accuracy,good precision and low detection limit.It can simultaneously determine the content of multiple components in gypsum,and provide certain technical support for the comprehensive utilization of gypsum resources investigation and evaluation.

关 键 词：电感耦合等离子体原子发射光谱法 偏硼酸锂-四硼酸锂 石膏 多组分分析 

分 类 号：O657.31[理学—分析化学] TH744.11[理学—化学]